CN111732118B

CN111732118B - Method for treating galaxolide musk waste aluminum salt water

Info

Publication number: CN111732118B
Application number: CN202010704404.4A
Authority: CN
Inventors: 程光锦; 易建康; 吕祖鹏; 方智中
Original assignee: Anhui Jinxuan Technology Co ltd
Current assignee: Anhui Jinxuan Technology Co ltd
Priority date: 2020-07-21
Filing date: 2020-07-21
Publication date: 2022-05-31
Anticipated expiration: 2040-07-21
Also published as: CN111732118A

Abstract

The invention relates to a method for treating galaxolide waste aluminum salt water, which is characterized by comprising the following steps: (1) continuously feeding the galaxolide waste aluminum salt water into an evaporation kettle, heating to 60-90 ℃ for evaporation, and condensing and recovering methanol gas obtained by evaporation; (2) after removing methanol, reducing the temperature of the evaporation kettle to 10-25 ℃, adding an extracting agent chlorobenzene into the evaporation kettle for extraction to remove heavy components, and controlling the mass ratio of the waste aluminum salt water to the chlorobenzene to be 5-10: 1; (3) after extraction, pumping the chlorobenzene phase on the upper layer to an extractant tank for evaporating and recovering chlorobenzene; and (3) utilizing the azeotropic principle to control the azeotropic temperature at 90-95 ℃ to evaporate the trace extracting agent and water in an azeotropic manner to obtain the finished polyaluminium water. The invention has the advantages that: the three wastes are reduced, and the waste aluminum salt water is prepared into qualified polyaluminium chloride water, so that the production cost is reduced; the reaction efficiency and the material utilization rate of the whole production flow are optimized, and the economic benefit of enterprises is increased.

Description

Method for treating galaxolide musk waste aluminum salt water

Technical Field

The invention belongs to the technical field of chemical production, and relates to a method for treating galaxolide waste aluminum salt water.

Background

Galaxolide is the first synthetic musk developed successfully in 60 s by international perfumery and flavor (IFF), with molecular weight of 258.4, boiling point of 129 ℃ (107Pa), chemical name of 1,3,4,6,7, 8-hexahydro-4, 6,6,7,8, 8-hexamethylcyclopenta-gamma-2-benzopyran, with strong and persistent musk aroma and woody aroma, and is widely used in the industries of cosmetics, soap essence, etc.

In the actual industrial production of galaxolide, 1 molecule of hexamethylindanol (GLA) and 1 molecule of methylal react under the catalysis of an aluminum trichloride/chlorobenzene solvent to generate 1 molecule of galaxolide and 2 molecules of methanol, then a large amount of water is added into a reaction solution to remove the methanol and the aluminum trichloride, and lower-layer waste aluminum salt water (methanol, polyaluminium, hydrochloric acid, water and aluminum chloride) is separated to obtain an upper-layer galaxolide crude product liquid.

The yield of waste aluminum salt water in the production of the galaxolide is large, one ton of galaxolide generates about 3 tons of waste aluminum salt water, if the waste aluminum salt water is evaporated (evaporated, concentrated and crystallized to obtain salt) by a conventional method, 3 tons of steam are needed, and then about 1 ton more aluminum salt paste is obtained; according to 200 yuan/ton steam, 600 yuan is needed, 1 ton of aluminum salt paste is sent with solid waste quality and transportation cost according to 5000 yuan/ton solid waste salt, the treatment cost reaches 6000 yuan, organic matters in the galaxolide must be removed due to the development of the galaxolide product which is greatly influenced, and the qualified polyaluminium water flocculant is obtained by changing waste into valuable.

Disclosure of Invention

The invention provides a method for treating waste aluminum salt water of galaxolide, which aims to purify the waste aluminum salt water in the reaction of synthesizing galaxolide to obtain qualified polyaluminum water.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a method for treating waste aluminum salt water of galaxolide is characterized by comprising the following steps:

(1) jewel musk waste aluminium salt water (methanol 4-6%, Sai Al)₂O₃7-9 percent of national standard polyaluminium chloride water, 0.05-1.5 percent of hydrochloric acid and 0.05-1.5 percent of chlorobenzene are continuously injected into an evaporation kettle, the temperature is raised to 60-90 ℃ for evaporation, and methanol gas obtained by evaporation is condensed (-10-30 ℃) and recovered;

2) after removing methanol, reducing the temperature of the evaporation kettle to 10-25 ℃, adding an extracting agent chlorobenzene into the evaporation kettle for extraction to remove heavy components, and controlling the mass ratio of the waste aluminum salt water to the chlorobenzene to be 5-10: 1;

3) after extraction, pumping the chlorobenzene phase on the upper layer to an extractant tank for evaporating and recovering chlorobenzene; and (3) utilizing the azeotropic principle to control the azeotropic temperature at 90-95 ℃ in the lower polyaluminium water phase, and azeotropically distilling out trace extractant and water to finally obtain the finished polyaluminium water (the content of aluminum oxide is 11%, and the COD is less than 500).

The invention has the advantages that: the three wastes are reduced, and the waste aluminum salt water is prepared into qualified polyaluminium water, so that the production cost is reduced; the reaction efficiency and the material utilization rate of the whole production flow are optimized, and the economic benefit of enterprises is increased.

The qualified polyaluminium water can be sold to a sewage station to be used as a flocculating agent according to the aluminium content, the price of the aluminium content of each 1 percent is 20 yuan, the price of the aluminium content of each 11 percent contains 220 yuan per ton, 3 tons of the polyaluminium water are produced by producing one ton of Jiale musk, 660 yuan is saved by producing one ton of Jiale musk, and the cost is reduced by nearly 1.5 percent according to the calculation of 4 ten thousand costs of Jiale musk. If the method is not adopted for treatment, and the treatment cost of 3 tons of the water as the waste brine needs 6000 yuan, the method for recovering the waste aluminum brine actually saves about 7600 yuan.

Drawings

FIG. 1 is a schematic process flow diagram of the present invention.

Detailed Description

The invention is further explained by combining figure 1, and the processing method of the galaxolide waste aluminum salt water comprises the following specific implementation steps:

example 1

1. Opening a feeding valve of an evaporation kettle, starting a feeding pump, pumping 6.5t of the galaxolide musk waste aluminum salt water into the evaporation kettle, starting steam, heating to 90 ℃, continuously condensing (20 ℃) waste methanol gas by a condenser for recycling during the heating, and finishing light component removal after no obvious liquid downflow is seen in a sight glass of the condenser to obtain 500kg of light components (65% of methanol);

2. after the light components are removed, cooling the interior of an evaporation kettle to 10 ℃, pumping 1 ton of chlorobenzene extractant into the evaporation kettle, stirring for 2 hours, standing for 2 hours, pumping the upper chlorobenzene phase to a chlorobenzene storage tank, and keeping the lower aluminum waste brine in the evaporation kettle;

3. Opening stirring, opening steam, slowly heating the evaporation kettle to 90 ℃, starting azeotropic distillation, condensing the brought chlorobenzene/water gas and then sending the condensed chlorobenzene/water gas to a water separation tank; when the temperature of the evaporation kettle rises to 95 ℃, closing steam, starting circulating water, cooling the evaporation kettle to normal temperature, and putting the aluminum water (with the content of aluminum oxide being 11 percent and COD 500) in the evaporation kettle into the polyaluminium water tank.

Example 2

1. Opening a feeding valve of an evaporation kettle, starting a feeding pump, pumping 6.5t of the galaxolide musk waste aluminum salt water into the evaporation kettle, starting steam, heating to 95 ℃, continuously condensing (10 ℃) waste methanol gas by a condenser for recycling during the heating, and finishing light component removal after no obvious liquid downflow is seen in a sight glass of the condenser to obtain 600kg of light component (65% of methanol);

2. after the light components are removed, cooling the interior of the evaporation kettle to 10 ℃, pumping 1.5 tons of chlorobenzene extractant into the evaporation kettle, stirring for 2 hours, standing for 2 hours, pumping the upper chlorobenzene phase to a chlorobenzene storage tank, and keeping the lower aluminum water in the evaporation kettle;

3. opening stirring, opening steam, slowly heating the evaporation kettle to 95 ℃, starting azeotropic distillation, condensing the brought chlorobenzene/water gas and then sending the condensed chlorobenzene/water gas to a water separation tank; when the temperature of the evaporation kettle rises to 100 ℃, closing steam, starting circulating water, cooling the evaporation kettle to normal temperature, and putting the aluminum water (with the content of aluminum oxide being 11 percent and COD being 400 percent) in the evaporation kettle into the polyaluminium water tank.

The foregoing is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting thereof in any way; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.

Claims

1. A method for treating waste aluminum salt water of galaxolide is characterized by comprising the following steps:

(1) continuously pumping the galaxolide waste aluminum salt water into an evaporation kettle, heating to 60-90 ℃ for evaporation, and condensing and recovering methanol gas obtained by evaporation;

(2) after removing methanol, reducing the temperature of the evaporation kettle to 10-25 ℃, adding an extracting agent chlorobenzene into the evaporation kettle for extraction to remove heavy components, and controlling the mass ratio of the waste aluminum salt water to the chlorobenzene to be 5-10: 1;

(3) after extraction, pumping the chlorobenzene phase on the upper layer to an extractant tank for evaporating and recovering chlorobenzene; heating the lower polyaluminium water phase to 90-95 ℃, and azeotropically evaporating trace amount of extractant and water to obtain finished polyaluminium water;

The galaxolide waste aluminum salt water contains 4-6% of methanol and Al₂O₃7-9%, hydrochloric acid 0.05-1.5%, chlorobenzene 0.05-1.5%;

the content of the polyaluminium hydrated alumina in the finished product is 11 percent, and the COD is less than 500.